Moriz weinbich



M. WEINRICH.

METHOD OF MANUFACTURING CARBONACEOUS FILTERING MEDIUMS.

APPLlCATION FILED JUNEZI! IQIU- 1,308,826. Patented July 8, 1919.

v I Inv-entqr: firg .lmorney.

U I ED STATESPATENT MORIZ WEINRICH, OF YONKERS, NEW YORK I METHOD or mnurecrumne To all whom it may concern:

Be it known that I, MORIZ Wnmmori, a citizen of the United States, residing at Yonkers, inthe county of Westchester and State of New York, have invented certain new and useful Imprdvements in Methods of Manufacturing Carbonaceous Filtering Mediums, of which the following is a specification.

My invention relates to a certain new and useful method of manufacturing carbonaceous filtering media and the invention consists of the method more particularly pointed out in the appended claims.

The object of the present invention is the manufacture of carbonaceous filtering materials from molasses, beet or cane molasses, or other impure or pure vegetable solutions containing sucrose or glucose, or both, and finely powdered lime, either caustic or hydrated, to which in some instances, finely powdered materials, insoluble in water, like 'hosphate of lime, fullers earth, kaolin, fire clay or other cla s, ki'eselguhr, etc., or mixtures thereof, shal be added. 'An intimate and uniform mixing of the molasses or other vegetable solutions with the finely powdered lime, or ime and some of the other named materials, is of prime importance and in order that my process may be better understood, I have illustrated in the drawing a type of apparatus which may be used and wherein the gure illustrates a sectional view partially in elevation of a mixer in the form of a closed vessel having appropriate mixing agencies; but it will be understood that the invention is not limited to i .this or to any other type of apparatus and that the apparatus is illustrated merely to disclose one embodiment of mechanism which may be used for effecting the intimate and uniform mixing of the solutions and ingredients before mentioned. To attain this result I may proceed substantially as follows:

(a) When using caustic powdered lime the molasses or other vegetable solutions, shall be unheated and have a density of about 75 Brix and the amount of hme powder used shall be about 30% of the weight of the solution to which shall be added about 20% of finely powdered dry slaked lime.

In the aforesaid drawing, A, is a closed vessel of appropriate size and construction, preferably cylindrical, having within 1t a oF IoE.

CARBONACEOUS FILTERING HEDIUMS.

Specification of Letters Patent.

Application filed June 21, 1918. Serial No. 241,192.

Patented July 8, 1919.

suitable stirring mechanism which may include "the arms, b, "fixed to a revolubly mounted shaft 12', and operatingin conjunction with other and stationar arms, a, fixed to the inside of the vessel. onnecting with oneend of the vessel are two inlets, through one of which, d, the solution is introduced in measured quantities and through theother, d, the lime'powder or a mixture of lime powder and some of the other named materials, is admitted, also in measured charges or quantities. The vertical shaft has means, as a pulley, through which power is applied to rotate the stirrer arms, 6, and by maintaining the cylinder or vessel A substantially full an intimate admixture of the solution and the powdered material is effected. In the op osite or lower end of the cylinder or vesse, A, is a gate-controlled outlet, e,"-through which the mixed mass is allowed to run in receptacles, B, whose four sides have a draft-toward the top, holding about two cubic feet each. They shall be filled to about 3 inches below their to and then removed to a warmed room. efore these receptacles are filled their inside shall receive a thin coat of some lubricant, so that the mass will discharge easily when hardened. After a while the caustic lime will combine with the water of the solution and at the same time with any sucrose, which may be in the solution, forming with it a sucrate of lime. By combining with the water of the solution heat is developed and the whole. mass will rise several inches and become hard but quite porous. The lime will decompose any glucose present but in doing so it will form likewise a very porous mass with it. The reason for using in this case a mixture of caustic and dry slaked lime is that if the whole amount of lime would be in the caustic state its action on the water contents of the solution would be too violent which might cause the burning of the whole mass.

. When mixing with the solution a mixture of lime powder and powdered insoluble material, the solution shall be thinned to about 65 Brix and the proportion of the materials shall be about as follows:

100 weighed parts of a 65 Brix solution.

25 weighed parts of powdered caustic lime.

60 weighed parts of any of the other in soluble materials.

The lime used shall be freshly burned and ground; into an impalpable powder. It is preferably burned in a kiln connected with the manufacturin plant since the carbonic acid gas, generated in the kiln, shall be likewise used with this process, as explained fur-. ther down.

Another method of obtaining the deslred results, may be stated as follows:

b) When using dry slaked, powdered lime alone the solution shall be brought to, or near to boiling and when of a density of about Brix about 60% of dry slaked lime of the weight of the solution shall be mixed into it in the same way as specified above. The lime will, at this temperature, likewise combine with any sucrose present in the solution 'to a sucrate of lime and will likewise decompose any glucose present. The by. drated lime will, however, not cause a risin and subsequent porosity of the mass butwi harden into a dry, lassymass.

When using ad 1t1onal powdered materials, mentioned above, the proportion of the various materials shall be about as follows:

100 weighed parts of a 65 Brix solution, heated to about boiling. 1 d 33 weighed parts of dry slaked lime pow- 60-weighed parts of any of the other insoluble materials.

Instead of dry hydrated lime a paste or a thick milk of lime may be used. In this case the solution has to be brought previously, when using lime alone, to at least Em; and when usin besides some of the other materials it sha 1 be kept at about 85 Brix in order to Secure the desired hard, glassy mass, which can be broken up easily into small pieces.

The mass in the receptacles will in both cases, of a mixture of caustic and dry slaked lime or hydrated lime alone be used, harden and dry within twenty-four hours, when they will be easily discharged by turning them over.

The mass is now broken up by suitable devices into small ieces. --Any dust formed may be either taken back into the mixing apparatus or may be treated further together with the small pieces.

The material shall pass now to an approriate drier, which may be heated by waste mace gases, in which drier it shall be thoroughly dried.

When comminuted and dried in this way it undergoes now in kilns, of similar construction as those used in the manufacture of bone-black, the process of dry distillation. The escaping gases are to be utilized in the well known wa by condensation. They will produce methy -alcohol, aceticacid, acetone, and a tar of peculiar odor and the proceeds from these products will cover a large portion of the working expenses.

When distillation is completed the prodsolution. For this purpose the pieces shall be dumped into a mixer equipped with a steam jacket and a double row of close] set mixing arms, the mixer having been lled previously with boiling water. The pieces will be broken up by the mixlng arms into small particles while the boiling water will dissolve a part of the lime.

inds of carbonaceous filtering v The material is kept for 5 or 10 minutes in 7 this mixer and then run into centrifugal ma chines lined with filter cloth and washed with additional boiling water. It 1s then dumped into receptacles where it is boiled with dilute hydrochloric acid until all the remaining lime has been dissolved. It is then again run into centrifugals, lined with filter cloth, washed with hot water and then sit steamed. After steaming the centrifu a1 isallowed to'operate'for 5 to 10 minutes w ereby the carbon will be dried. It is then removed from the centrifugals and is ready for use. Its decolorizing ower in the filtra tion of sugar, glucose, an other solutions. or oils is very great. Besides, it could be used to advantage in the manufacture of high grade printers ink.

The second way is to convert the lime into carbonate of lime. To attain this the pieces,

after having left the retorts and having been cooled, shall be put into a vessel provided with a perforated false bottom. It

is now washed with cold water, slightly acidulated with hydrochloric acid, in order to wash off any fine particles of lime, which I may have settled on the surface of the material. This acidulated water shall be now followed 'by enough pure cold water to cover the mass for several feet and carbonic acid gas from the lime kiln, or, if not connected with the plant, from some other source, shall be pumped beneath this perforated bottom. The gas will penetrate into the pieces and combine with the free lime present into carbonate of lime, which is insoluble in water,

increasing thereby also the weight of the material. Or the false bottom may be placed in the upper part of the vessel and the cooled materia1, coming from the retorts, shall be put in its dry state on this false bottom. The space beneath the false bottom is partly filled with water, kept hot or boiling by steam injection. The carbonic acid-gas is pumped into this water so that the escaping gas, mingled with the vapors from the hot water, will penetrate through the perforations of the false bottom into the material phosphate of lime.

and convert it's free lime contents into carbonate of lime. As soon as this has been accomplished the material may be Washed in the same vessel with boiling water remov- 5 ing soluble impurities, then taken out and dried in some suitable drying device, when it will be ready for use.

Instead of converting the free lime into carbonate of lime,it maybe converted, after 10 the material has been washed with acidulated water, into phosphate: of lime. In this case the material is dumped into a vessel containing a hot solution of phosphoric acid strong enough to convert the free lime into It is then taken out washed with boiling water and dried. I

refer, however, generally the use of caronic acid because it costs nothing When a lime kiln is connected with the plant.

When manufacturing mixtures containing besides lime any of the above mentioned finely powdered insoluble materials, the pieces after having left the retorts shall be treated in the same way with carbonic acid gas or a phosphoric acid solution. It will then make a cheap and efiective substitute for bone-black. After each use the material can be revivified to good advantage by gentle oxidation according to my rocess and apparatuses covered by my U. patents of December 15, 1914, Number 1,121,429; of May 2-3, 1916,.Number 1,185,397; and of May 23, 1916, Number 1,184,398.

The lime or limestone used with this process shall be of the same quality as that .used generally in the sugar industry and may contain a few per cent. of impurities as silica, alumina and magnesia.

The revivification of pure carbon when 4o-used for filtering purposes is done best and cheapest by bOlllIlg it in closed vessels, equipped with a condenser for condensing escaping vapors, in an ammonia solution. The ammonla will dissolve the impurities and coloring matter taken up by the carbon and will then escape with the water vapors with which'it will be'condensed and used over and over again. The material is then run with the remaining water into filter presses and washed therein with hot water when it is again ready for use.

Having thus described my invention what I claim as new and desire to secure by Letters Patent is 1. The-manufacture of carbonaceous filtering media consisting in mixing solutions containing sucrose or glucose or both with lime in such proportions and at such temperatures that a chemical combination of the lime and sucrose or glucose will take place obtaining a hard mam; c'ommlnuting this mass; then calcining the mass; then cooling the burnt material and then 'reparing the same for filtering media, sui antially as set forth.

2. The manufacture of carbonaceous filtering media consisting in mixing solutions containing sucrose or glucose or both with lime in such proportions and at such temperatures that a chemical combination of the lime and sucrose or glucose will take place obtainmg a hard mass; comminuting this mass; then calcining the'mass; then cooling the burnt 'material, and finally converting its free lime contents by means of some suitable acid into a calcium-salt insoluble in water.

3. The manufacture of carbonaceous filtering media consisting in mixing solutions 

